Monolithic supports and methods for their production
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example 1
Bulk Monolith Preparation
[0061]Polyamide solutions were prepared by dissolving ˜120-190 mg of each polyamide in 1 g benzyl alcohol. The dissolution took place in 1.5 ml borosilicate vials sealed with PTFE-faced septa and crimp caps for varying periods of time. During the dissolution, the vials were immersed in a sand bath that was placed in a convective laboratory oven (Electrolux, SE), where the temperature measured over time and at different spots in the sand bath varied from 150-160°. This temperature variation was mainly due to frequent opening of the oven to carry out the mixing cycles, which consisted of a gentle manual shake for 5-10 s every 30 min in order to facilitate the dissolution of the swollen polymer. After 4-5 shaking cycles the solutions appeared homogenous and were then left unstirred in the sand bath for up to 48 h to ascertain complete dissolution. The solutions were then allowed to cool slowly to room temperature by turning off the oven with the vials still sub...
example 2
Capillary Monolith Preparation
[0062]Method:
[0063]For the capillary column format, the capillaries were pre-treated, firstly by etching with 1 M aqueous NaOH for 2 h, then thoroughly washed in sequence with water and dried acetone, and finally dried with nitrogen gas. The dry activated capillaries were then reacted with 3-glycidoxypropyl trimethoxy silane in dried toluene (1:4 v / v) at 110° C. for 6 h, with following toluene and acetone washing steps. The polyamide solutions for the capillary experiments were prepared in the same way as above, with a total heating time of about 3 h. Directly upon removal from the oven and while still in the sand bath, the polymer solutions were flushed from the glass vials into the capillaries by piercing the septum with a piece of unheated capillary and compressed helium supplied through a hypodermic needle was used to propel several capillary volumes of the solution from the vial into the capillary, at a rate fast enough to heat the capillary during...
example 3
Surface Area Determination
[0067]The specific surface area was determined by nitrogen adsorption-desorption on a Micrometrics (Norcross, Ga., US) Tristar 3000 automated gas adsorption analyzer, measuring multipoint surface area and average pore width of the particles based on the Brunauer-Emmett-Teller equation (Brunauer, S., The Adsorption of Gases and Vapors. I. Physical Adsorption., Princeton University Press, Princeton, 1945). The Tristar 3000 was also used to calculate the total pore volume of the particles by measuring N2 adsorption close to atmospheric pressure. Before analysis the monolithic cubes were dried in a vacuum oven at 40° C. overnight to remove adsorbed gases from the pores. Approximately 100 mg of material was placed in a sample tube and dried again before analysis at 120° C. for at least 3 hours under continuous nitrogen flow, using a Micrometrics SmartPrep degassing unit. Results can be found in table 1. It was found that the materials with more or less rod-type ...
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